In this slide contains Infrared-Spectroscopy (IR) in Pre-Formulations and various uses. Presented by: B. Venkatesh. ( Department of pharmaceutics) RIPRE,anantpur.

1. RIPER
AUTONOMOUS
NAAC &
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SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1
Infrared-Spectroscopy (IR)
in Pre-formulations
1
A Seminar as a part of curricular requirement
for I year M. Pharm I semester
Presented by
Mr B Venkatesh
(Reg. No. 20L81S0301)
Under the guidance/Mentorship of
Dr CH Pavan Kumar., M. Pharm., PhD
Associate Professor & Head
Dept. of Pharmaceutics

2. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2
Contents
• Glance at Pre-formulation
• About IR spectroscopy
• How to read IR Spectra?
• Various uses of IR Spectra in pre-formulations
• References
2

3. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
Glance at Pre-formulation
• Pre-formulation studies are initial stage of product
development, and considered as formulation research.
• Here, physico-chemical properties of drug substance (API) are
considered to optimise and,
• to recommend the suitable dosage form for human studies
(Clinical Trial). As per regulatory requirements (FDA), pre-
formulation studies is focused to achieve,
• Efficacy & Safety
• Stability & storage conditions
• Suitable packaging material.
3

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Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4
About IR spectroscopy
4
IR spectroscopy is based on absorption of mid infrared
region (4000-400cm-1) by chemical bonds in an organic
compound,
It results IR spectra, % transmittance (y-axis) and
wavenumber (x-axis).
Mid-IR Ray

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Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5
How to read IR Spectra?
5
• Each peak indicates functional group /
bond of a compound.
• Thus, peak positions are the
characteristic of any drug or chemical
entity. Absorbance mode
Transmission mode
• Both, transmission and absorbance
mode are used in interpretation of IR
spectra.
• From overlay spectra, we can easily
differentiate the distinct character of
different compounds/API/formulations.

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Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6
Various uses of IR Spectra
in pre-formulations
6
a) Identification of drug in formulations
b) Identification of additives in dosage forms
c) Detection of drug - excipients compatibilities
d) Detection of drug Polymorphism
e) Detection of drug stability in formulations
f) Confirmation of soluble complex of drug with polymer
g) Characterization of Nano-formulation
i. Nanoparticles
ii. Liposomes
iii. Niosomes
h) Characterization of microsphere
i) Characterization of formulation with physical mixture

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K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7
a) Identification of drug in formulations
7

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K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8
b) Identification of additives in dosage
forms
8

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K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9
c) Detection of drug - excipients
compatibilities
9
• Comparison of IR spectra indicates the drug, formulation & placebo.
• It suggests the
possible in chemical
interactions between
Drug and excipient
• Usually, the shift of
band for OH, NH, SH,
C=O, S=O are
considered to be
significant for
interactions.

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Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10
d) Detection of drug Polymorphism
10
• Polymorphism of
a drug
characterized by
peak position,
peak intensity
and peak width.
• The significant
changes in above
parameters
indicates the
changes in
polymorphism

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K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11
e) Detection of drug stability
in formulations
11
• FT-IR spectra of ibuprofen (IB) (blue) and after subtracting of the spectrum
of the mixture of the 4 excipients from formulation (green).
• In the frame the enlarged zone of the fingerprint region of standard IB and
of the residual spectra.

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K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12
f) Confirmation of soluble complex of
drug with polymer
12
The FTIR spectrum of (a) natamycin,
(b) Methyl-β-Cyclodextrin (ME-β-
CD), and (c) natamycin/ME-β-CD
inclusion complex.
• Compared with the spectrum of pure
ME-β -CD, a new small peak at 1717
cm−1 can be found for the complex.
• As noted above, the conjugated ester
absorption band (1716 cm −1 ) is the
most informative one and appears for
natamycin

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K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13
g) Characterization of Nano-formulations
13
FTIR spectra of Chitosan nanoparticles with
tripolyphosphate and Chitosan .
• These peaks shift to 1639
and 1557 cm-1 in the FTIR
spectra of C=N which
caused by the interaction
between NH3 + groups of
chitosan and phosphate
groups of TPP.
• This interaction is also
supported by the
decrease of amide band I
(1639 cm-1) intensity in
CN compared to CS.
i. Nano particles:

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14
FT-IR infrared spectra of
pure PEG-2000 (black)
and PEGylated liposomal
wedelolactone (Red)
ii. Liposomes:

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FT-IR spectra of vancomycin hydrochloride free drug (A), unloaded
niosomes (B) and vancomycin loaded niosomes (C)
iii. Niosomes:

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FT-IR spectra of (A) pure esomeprazole magnesium and (B) microsphere
formulation.
h) Characterization of microsphere

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(i) Band between 3250 cm–1 and 3260
cm–1 was observed instead of a
sharp peak at 3269 cm–1 in case of
Meloxicam (MLX);
(ii) Disappearance of band at 2920 cm–
1 which specified for CONH group in
case of pure MLX, and
(iii) Shifting of band 1089 cm–1 (Si–O
stretching vibrations of Silica MCM-
41 into 1075 cm–1.
(iv) The majority of the MCM-41
isolated terminal silanol groups in
F2 interacted with MLX molecules.
i)Characterization of formulation
and physical mixture

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K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 18
References
18
1. Ramalingam Pearman and Y Padmanabhan Reddy, Application of spectral studies
in Pharmaceutical Product Development, 1st Edition, Hyderabad (India),
PharmaMed Press, 2019.
2. Stefanos Mourdikoudis, Roger M. Pallares and Nguyen T. K.
Thanh, Characterization techniques for nanoparticles: comparison and
complementarity upon studying nanoparticle properties, Nanoscale, 2018, 10,
12871-12934.
3. John L. Koontz, Joseph E. Marcy, Formation of Natamycin : Cyclodextrin
Inclusion Complexes and Their Characterization, J. Agric. Food Chem. 2003, 51,
24, 7106–7110.
4. Felicia Dragan, Irina Kacso, Simina Dreve, Flavia Martin, Gheorghe Borodi, Ioan
Bratu, Kamel Earar, Compatibility Study of Ibuprofen with Some Excipients
Employed for Solid Dosage Forms, REV. CHIM. (Bucharest), 2015, 66(2), 191-
195.

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Thank you